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ec. 4, ma.

G. E. JENKS PRO CESS OF REFINING WOOD ROSI N Filed May 15, 1923 2 Sheets-Sheet TO VACUUM CON DENSE R ROSB N POT W/T/YEES.

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Dec. 4, 1928.

G. E. JENKS PROCESS OF REFINING WOOD ROSIN Filed May 15, 1925 2 Sheets-Sheet 2 VVENTO? Gywy f da/%3 W/TNESS:

Patented Dec. 4:, tere tmiren srsrss GEORGE E. JENE& OF BACGHUS, UTAI-l, ASSIGNOE TO HERCULES POVVDER COMPANY, OF WIEMINGTON, DELAWABE, A COEIPOEATION OF DELAVTAEE;

IPIROCESS OF R'EFINIEIG WOOD ROSIN.

Application filed May 15,

The object of my invention is to so treat Wood rosin as to produce a rosn so highly refined that it is adapted for use in sizmg the higher grades of paper, inthe manufacture ot better grades o' varnish and tor other purposes for which a high grade rosn s adapted.

A known process of producing Wood rosn of a lower grade, and the process that Ipref erably employ as a preliminery process in the manufacture of more highly refined ros1n consists in grnding .Wood and sturops from pine trees, placing the Wood stock n large digesters, passing s'teani through the stock and thus driving off a considerable quant ty of turpentine, flooding the stock With gasolne or other solvent, thereby extracting certain materials, chiefly rosin, pine oil and var ous color bodies, passing the gasoline solution, commonly 'known as drop liquor, through suitable evaporators, and fractionally remov+ ing the gasoline and pine oil. The pine oil produced by the distillation s reined and sold. The recovered gasoli'ne is again used in the process The recovered rosn is e niarketable product, but is setist'actory tor slzing only the lower grades of paper and in making the 1nterior grades of varnish, and therefore must be narlzeted at e relativelylow price.

A process has been-developed by Harry E. Kaiser and Arthur langrneier, 'for which. they filed an application for patent on the fitteenth day ot lvlay1923, Serial No. 639,()5& whereby the lower grade rosin is subjected to a treatment that greatly iinproves the color of the rosin and iniparts to it generally such high quality, both cheznical and physical, as to adapt it for sizing the higher grades ot paper and for use in the better grades of varnish. T have so ii'nproved the main distillation step of this process as to recover a larger proportion Ott rosin in the subsequent fractional condensation. In order that my inventon may be understood, 'it Will be neces sary to describe the above 'n'entioned Kaiser and Langneer' process to which my invention is applicable. It is also necessary to carry out, at least in part the said process' in order to practice the process involving my invention. T shall, therefore, describe the, entire process as improved by nie and particularly point out that modification of the process involvng my invention.

Tosecure the best results, it is preferred 1923. Serial Ne. 639,()64.

to preliminarily distill the rosin to remove seine of the objectionable coloring matter;

and any rosin and rosin oil Vapors or mist' that pass' over the fractional condensers and that, if condensed in the vacuum lines, Would clog them up and prevent regular operation.

In the above described processthe rosin in the main still` is under vacuuin and is preterably heated by means of hot oil fiowing through 'tubes With Which the rosin is brought into contact or contained in a jacket surrounding a body of rosin. I have discovered that a lar 'er proportion of the rosin can be recovered by injecting into the rosin superheated stcan at a temperature approximating the temperature that it is desired to maintain in the still. The superheated steam lowers the temperature of distillation.` To secure the degree of hezt desired, an independent, heating medium, such as the hot oil described, should be used.

'In the drawings, which illustrate .apperatus for carrying out the major part of the entire process, in its preferable embodiment- 4 Fig. lis a diagrammatic View, in elevation, of that part of the complete rosin refining apparatus comprsing the preheater and still. i

Fg. 1 is a similar View of the remainder ot the apparatus, comprisng the fractional condensers and scrubbers.

The rosin is first heetedsin a preheater a having `a vacuum connection b by Way of a small condenser c. The preheater may be effectively heated by means of a coil d through which heated oil is circulated. There are two automatic feeds, one e into the preheater and the other f from the'preheater to 'the still. The rosi'n should be heated in the preheater to a temperature oi' about 480 F. By'preheating the rosin, any low boiling coloring mat-ter that may be in the rosin as it is introduced into the system is taken oti' and condensed As different rosins have Varying proportions of this low boiling coloring matter, the preliminary distillation will insure substantial nniformity in the .material th at passes to main still.

i: the

The still g is perterably lined with alu-.

heated in batch by means ot a jacket kt, sur-' roundng the still, through whichthe heated oil circulates, z' being the oil inlet and the oil outlet. 'The superheated steam is introduced by means ot' a steam pipe m. The steam is injected into the body of the rosin. The steam should be at a temperature approximating the temperature hat itis desired to maintain in the still.

The rosin should be heated at. a temperature well over 500 F. and preferably about 600 or 650 F. The bottom of the still is connected with a Vessel 73 to receive the residue.

The rosin vapors are carried oli by a pipe Z through a succession of fractional condensers, which may be of any number, preferably three or four. Three are shown and marked n, 0 and p. Each condenser is maintained at a predetermined temperature by means ot surrounding acket g( in which hoat-ed oil is circulated. lt is preferred to maintain' three condensers n, 0 and p (where three are used) at temperatures of 400 F., 350 F. and 300 F. respectively.

A high degree of Vacuum seems essential to successful rosin distillation. A vacuum of v twenty-eight inches of mercury column (it is of excellent color and of such high quality,

both physically and chemically, that it can be used for sizinc' the highest grade paper, for making the best Varnish, and for other purposes. The rosin condensed in the second condenser 0 is of good quality and commands a substantially higher price tham the rosin introduced into the system. The rosin condensed in `the last condenser is inferor in quality to that condensed in the other condensers. To produce really high grade rosin, the temperature ot the condenser should not be less than 350 F. and should be nearer 400 F. At this temperature is produced a water-tree product comparativcly tree from rosin oil and pine oil, and there is little danger of the condensel rosin crystallizing. By increasing the number of condensers or by heating i fercnt 'from the temperaturcs heroin speci-- fied,'or by both means, a smaller proportion of theyery highest grade rosin, or ala 'ger proportion of rosin of somewhat lower, but still high, grade may be secured. The number ot condensers and the temperature regulation will depend upon the grade of rosin that it is desired to obtan and particularly the purpose for which the rosin is intended to be used.

The rosin and rosin oil Vapors that escape from the last condenser pass to the solvcnt scrubber shown. These vapors, which are essentially a mixture of' rosin and rosin oil, probably do not amount to over two or three per cent of the rosin distilled. The Vapors pass through the return bend pipe condenser r, which is water-cooled by means of a distributor s. A recirculating stream of solvent gasoline or kerosene) is maintained inside ot the condenser pipes. lVithout this hydrocarbon solvent, the rosin that would condense in the pipes r would not be in suficient quantity or sufficiently fluid to flow freely. During' any single traverse of the condenser pipes, the solvent dissolves much less rosin and rosin Vapor than it is capable of absorbing, and it is theretore recirculated until it becomes saturated. The solution of hydrocarbon oil and rosin and rosin oil, mixed with water of condensation, passes to a solvent settling or separating tank t, wherein the water settles to the bottom and is withdrawn through the ValVed pipe u. The hydrocarbon oil, with rosin and rosin oil dissolved therein, overfiows into a pipe o and, by means of a pump w, is returned through 'a pipe w to the pipe condenser r. As the solvent becomes saturated it is replaced with fresh solvent. y

The vacuum in the apparatus may be maintained by connectng 'the settlng tank t, through pipe y, with Vacuum.

Having now fully described my invention, what I claim and desire to protect by Letters Patent is:

l. The process of refining wood rosin which comprises Vaporizing the same under a high Vacuum by the concurrent action of two heating media one of which is exteriorly appled and the other of which is superheated steam injected into the body of the rosin, and condensing a portion of the distillate at a temperature not less than about 350 F.

2. The process of refining wood rosin which comprises Vaporzing the same under a sie condensers to temperatures dithigh Vacuum by the concurreit action of two heating media one of which is exterioi'ly applied and the other of which is superheated steam injected into the body of the i'osin, and 'ractionally condensing the distillate at temperatures the highest of which does not substantally exceed 400 F.

3. The process of refining wood rosin which comprises p'eheating` the same at a temperature sufiiciently above its nielting point to drive off low boling coloring matter and condensing the same, said temperatures being maintained below that required to distill the -osin, and then heating the rosin to the sub* stantially higher temperature required to distll most of the rosin, said rosin-distilling temperature being esteblished and maintained by the concurrent action of two heating media one exteriorly applied and the other superheated steam injected into the body of the rosin; 3,11 of said Operations being co11 ducted under a high vaouum.

` In testimony of which invention, I have hereunto set my hand, at Bacchus, Utah, on this 18th day of April, 1923.

GEORGE E. J ENKS. 

